Method and apparatus for treating organosiloxane coating film

ABSTRACT

A method for processing an organosiloxane film includes loading a target substrate (W) with a coating film formed thereon into a reaction chamber ( 2 ), and performing a heat process on the target substrate (W) within the reaction chamber ( 2 ) to bake the coating film. The coating film contains a polysiloxane base solution having an organic functional group. The heat process includes a temperature setting step of setting an interior of the reaction chamber ( 2 ) at a process temperature by heating, and a supplying step of supplying a baking gas into the reaction chamber ( 2 ) set at the process temperature, while activating the baking gas by a gas activation section ( 14 ) disposed outside the reaction chamber ( 2 ).

TECHNICAL FIELD

The present invention relates to a method and apparatus for processingan organosiloxane film by performing a heat process on a targetsubstrate with a coating film of a polysiloxane base solution appliedthereon, thereby baking the coating film.

BACKGROUND ART

In order to increase the operational speed of LSIs, it is required todecrease the specific dielectric constant of inter-level insulatingfilms. As an inter-level insulating film with a low dielectric constant,an organosiloxane film is known. Where an organosiloxane film is formed,a coating film of a polysiloxane base solution having an organicfunctional group is first formed by spin coating on a target substrate,such as a semiconductor wafer. Then, a heat process (baking process) isperformed on the wafer to bake the coating film.

For example, Jpn. Pat. Appln. KOKAI Publication No. 2001-308089discloses a method of forming an organosiloxane film of this kind.According to this method, a process of baking a coating film isperformed at a temperature of, e.g., from 400 to 450° C. for about 30minutes. This baking process is performed within a nitrogen atmosphereto prevent organic functional groups from decomposing.

Jpn. Pat. Appln. KOKAI Publication No. 2003-158126 (published on May 30,2003), discloses an improved method of forming an organosiloxane film.According to this method, a catalytic gas, such as a mixture gas ofammonia and water, dinitrogen oxide gas, or hydrogen gas, is used in thebaking process. In this case, the process temperature can be lowered toa temperature of from 300 to 400° C.

DISCLOSURE OF INVENTION

An object of the present invention is to provide a method and apparatusfor processing an organosiloxane film, which allow an inter-levelinsulating film with a low dielectric constant to be formed at a lowheat-processing temperature.

According to a first aspect of the present invention, there is provideda method for processing an organosiloxane film, the method comprising:

loading a target substrate with a coating film formed thereon into areaction chamber, the coating film comprising a polysiloxane basesolution having an organic functional group; and

performing a heat process on the target substrate within the reactionchamber to bake the coating film,

wherein the heat process comprises

a temperature setting step of setting an interior of the reactionchamber at a process temperature by heating, and

a supplying step of supplying a baking gas into the reaction chamber setat the process temperature, while activating the baking gas by a gasactivation section disposed outside the reaction chamber.

According to a second aspect of the present invention, there is providedan apparatus for processing an organosiloxane film, by performing a heatprocess on a target substrate with a coating film formed thereon to bakethe coating film, the coating film comprising a polysiloxane basesolution having an organic functional group, the apparatus comprising:

a reaction chamber configured to accommodate the target substrate;

a temperature adjusting section configured to adjust temperature insidethe reaction chamber;

a gas supply section configured to supply a baking gas into the reactionchamber;

a gas activation section disposed outside the reaction chamber andconfigured to activate the baking gas;

an exhaust section configured to exhaust gas inside the reactionchamber; and

a control section configured to control the temperature adjustingsection, the gas supply section, the gas activation section, and theexhaust section.

BRIEF DESCRIPTION OF DRAWINGS

FIG. 1 is a sectional side view showing a vertical heat-processingapparatus according to an embodiment of the present invention;

FIG. 2 is a graph showing the relationship between the bakingtemperature (heat process temperature) and the specific dielectricconstant of a film formed in a case where ammonia gas was employed as abaking gas; and

FIG. 3 is a graph showing the relationship between the bakingtemperature (heat process temperature) and the specific dielectricconstant of a film formed in a case where dinitrogen oxide gas wasemployed as a baking gas.

BEST MODE FOR CARRYING OUT THE INVENTION

As the number of multi-layered interconnection lines is increased andthe structure is downsized in LSIs, inter-level insulating films usedtherein are required to have a lower dielectric constant property, andalso to be formed at a lower process temperature. The latter is intendedto alleviate the thermal history of a film earlier formed inmulti-layered structures, because such a film is subjected to heatprocesses repeatedly performed thereafter. Further, it is an ongoingrequirement to reduce the process time involved in semiconductormanufacturing. However, where the process temperature is lowered and theprocess time is shortened, a coating film may be insufficientlyheat-processed, thereby hindering formation of an inter-level insulatingfilm with a low dielectric constant.

Particularly, where a polysiloxane base solution is used along with alow process temperature and a short process time, formation of aninsulating film with a low dielectric constant becomes difficult. Thisproblem is thought to arise from the following mechanism. Specifically,the baking process (or heat process) is used to cause (—SiOH)'s presentin an applied coating solution to inter-react with each other, therebyproducing (—Si—O—Si—)'s. If the coating film is supplied withinsufficient thermal energy, the reaction described above cannotpropagate through the entire coating film. As a consequence, a largenumber of (—SiOH)'s remain in the film, which hinders the dielectricconstant from decreasing.

Embodiments of the present invention achieved on the basis of thefindings given above will now be described with reference to theaccompanying drawings.

FIG. 1 is a sectional side view showing a vertical heat-processingapparatus of the batch type according to an embodiment of the presentinvention. As shown in FIG. 1, the heat-processing apparatus 1 includesa reaction tube (reaction chamber) 2, which is essentially cylindricalwith a longitudinal direction directed in the vertical direction. Thereaction tube 2 has a double-tube structure formed of an inner tube 3and an outer tube 4 having a closed top, wherein the outer tube 4 coversthe inner tube 3 with a constant gap interposed therebetween. The innertube 3 and outer tube 4 are formed of a heat-resistant material, such asquartz.

A cylindrical manifold 5 made of stainless steel (SUS) is disposed belowthe outer tube 4. The manifold 5 is airtightly connected to the bottomof the outer tube 4. The inner tube 3 is supported by a support ring 6,which is integrally formed with the manifold 5 and extends from theinner wall of the manifold 5.

The manifold 5 is engaged with a lid 7 disposed therebelow, which ismoved up and down by a boat elevator 8. When the lid 7 is moved up bythe boat elevator 8, the bottom port of the manifold 5 is closed.

A wafer boat 9 made of, e.g., quartz is placed on the lid 7. The waferboat 9 is arranged to support a plurality of semiconductor wafers(target substrates) 10, at predetermined intervals in the verticaldirection. Each of the wafers 10 is provided with a coating film formedthereon. For example, the coating film consists of a coating solutioncontaining polysiloxane having an organic functional group, which hasbeen applied onto the semiconductor wafer 10 by spin coating. Thecoating film will be heat-processed (baked) by the heat-processingapparatus 1. As a consequence, an inter-level insulating film, such asan insulating film of polysiloxane having an organic functional group,which is an insulating film with a low dielectric constant, is formed onthe semiconductor wafer 10.

A heat-insulating structure 11 is disposed to surround the reaction tube2. The heat-insulating structure 11 is provided with a heater 12, suchas a resistance heating body, which is disposed on the inner wall of thestructure 11 and is used to raise the temperature. The interior of thereaction tube 2 is heated to a predetermined temperature by the heater12, so that the wafers 10 are heated to a predetermined temperature.

A baking gas feed line 13 for supplying a baking gas into the reactiontube 2 is inserted through the sidewall of the manifold 5. The bakinggas feed line 13 is connected to a predetermined baking gas supplysource (not shown) through a mass-flow controller (not shown) and soforth inside the gas supply section GS. For example, the baking gas maybe selected from ammonia gas, dinitrogen oxide gas, nitrogen oxide gas,hydrogen gas, argon gas, and nitrogen gas.

For example, as shown in FIG. 1, the baking gas feed line 13 is insertedthrough the sidewall of the manifold 5 at a position below the supportring 6 (below the inner tube 3). The baking gas feed line 13 is bentupward in the manifold 5 to face the interior of the inner tube 3 frombelow. In practice, a plurality of baking gas feed lines 13 aredisposed, but FIG. 1 depicts only one of them.

Furthermore, a purge gas feed line 16 for supplying a purge gas isconnected to the sidewall of the manifold 5. The purge gas feed line 16is connected to a predetermined purge gas supply source (not shown)through a mass-flow controller (not shown) and so forth inside the gassupply section GS. The purge gas may be exemplified by an inactive gas,such as nitrogen.

The baking gas feed line 13 is provided with an activation section 14disposed thereon for activating the baking gas. The activation section14 is arranged to activate the baking gas by means of heat, plasma,light, or catalyst, and thus includes, e.g., heating means, plasmageneration means, photolyzation means, or catalytic activation means. Inthis embodiment, the activation section 14 is formed of a heating deviceconfigured to heat the baking gas to a temperature for activation,raging, e.g., from 500 to 2000° C., and preferably 700 to 1000° C. Thebaking gas supplied from the baking gas supply source is heated andthereby activated by the heating device (activation section 14), andthis activated baking gas is supplied into the reaction tube 2.

The activation section 14 may be arranged to activate the baking gas bya combination of exciting medium energy with catalytic action. Forexample, the catalyst consists of tungsten, platinum, or titanium oxide.In this case, the baking gas comes into contact with the catalyst, whilebeing supplied with energy from a medium selected from the groupconsists of heat, light, and plasma. Where the activation section 14 ofthe heating device type shown in FIG. 1 is combined with a catalyst,catalytic pellets 14 a or the like may be contained in the heatingchamber, as indicated with broken lines in FIG. 1.

An exhaust port 15 is formed in the sidewall of the manifold 5 above thegas feed lines 13 and 16. The exhaust port 15 is formed above thesupport ring 6, and communicates with the space formed between the innertube 3 and outer tube 4 of the reaction tube 2. The exhaust gas or thelike generated inside the inner tube 3 is exhausted through the spaceformed between the inner tube 3 and outer tube 4 to the exhaust port 15.

The exhaust port 15 is airtightly connected to an exhaust line 17. Theexhaust line 17 is provided with a valve 18 and a vacuum pump 19disposed thereon in this order from the upstream side. The valve 18adjusts the opening ratio to control the pressure inside the reactiontube 2 to a predetermined pressure. The vacuum pump 19 exhausts gasinside the reaction tube 2 through the exhaust line 17, and therebyadjusts the pressure inside the reaction tube 2. The exhaust line 17 isprovided with a trap, a scrubber, and so forth (not shown) disposedthereon. The exhaust gas from the reaction tube 2 is detoxified and thenexhausted out of the heat-processing apparatus 1.

The boat elevator 8, temperature-raising heater 12, baking gas feed line13, activation section 14, purge gas feed line 16, valve 18, and vacuumpump 19 are controlled by a control section 20. The control section 20comprises a microprocessor, a process controller, and so forth.Temperatures and pressures at respective portions of the heat-processingapparatus 1 are measured and transmitted to the control section 20. Thecontrol section 20 outputs control signals or the like to the respectiveportions based on the measurement data to control them. As aconsequence, these portions of the heat-processing apparatus 1 arecontrolled in accordance with a predetermined recipe (time sequence).

Next, an explanation will be give of a heat-processing method, using theheat-processing apparatus 1 described above. This embodiment isexemplified by a method for processing an organosiloxane film. Insummary, a coating film of a polysiloxane base solution having anorganic functional group is formed by spin coating on a target substrateor semiconductor wafer. Then, the wafer is subjected to a heat process(baking process) to bake the coating film.

Specifically, a coating film of a polysiloxane base solution is formedon a semiconductor wafer by, e.g., spin coating and drying performedthereon. The solution contains a bond of a silicon atom with afunctional group selected from the group consisting of a methyl group(—CH₃), phenyl group (—C₆H₅), and vinyl group (—CH═CH₂).

The polysiloxane is prepared by hydrolyzing a silane compound having ahydrolyte group under the existence or non-existence of a catalyticagent to condense it. A preferable example of a silane compoundcontaining a hydrolyte group is trimethoxysilane, triethoxysilane,methyltrimethoxysilane, methyltriethoxysilane,methyltri-n-propoxysilane, methyltri-iso-propoxysilane,ethyltrimethoxysilane, ethyltriethoxysilane, vinyltrimethoxysilane,vinyltriethoxysilane, phenyltrimethoxysilane, phenyltriethoxysilane,dimethyldimethoxysilane, dimethyldiethoxysilane, diethyldimethoxysilane,diethyldiethoxysilane, diphenyldimethoxysilane, diphenyldiethoxysilane,tetramethoxysilane, tetraethoxysilane, tetra-n-propoxysilane,tetra-iso-propoxysilane, tetra-n-butoxysilane, tetra-sec-butoxysilane,tetra-tert-butoxysilane, or tetraphenoxysilane.

The catalytic agent used in hydrolysis may be an acid, chelate compound,or alkali, and is preferably an alkali, such as ammonia or alkylamine.

The molecular weight of polysiloxane is 100,000 to 10,000,000,preferably 100,000 to 9,000,000, and more preferably 200,000 to8,000,000 in weight-average molecular weight obtained by polystyreneconversion in accordance with a GPC method. Where it is less than50,000, the dielectric constant and elastic modulus may be insufficient.Where it is greater than 10,000,000, the uniformity of a coating filmmay be lowered.

It is preferable to use a polysiloxane base solution that satisfies thefollowing formula.

0.9≧R/Y≧0.2 (where R denotes the atomicity of the methyl group, phenylgroup, or vinyl group, and Y denotes the atomicity of Si, both inpolysiloxane).

The polysiloxane base solution (coating solution) is prepared bydissolving such polysiloxane into an organic solvent. A concrete exampleof a solvent to be used for this is at least one selected from the groupconsisting of an alcohol base solvent, ketone base solvent, amide basesolvent, and ester base solvent. In addition to polysiloxane, thecoating solution may contain an arbitrary component, such as asurfactant, or pyrolytic polymer, as needed.

A wafer 10 with a coating film thus formed thereon is subjected to aheat process by the heat-processing apparatus 1 in a sequence asfollows. In this sequence, the control section 20 controls respectiveportions of the heat-processing apparatus 1 explained below.

At first, the interior of the reaction tube 2 is heated by thetemperature-raising heater 12 at a predetermined baking temperature of,e.g., from 250 to 400° C. On the other hand, the wafer boat 9 holdingsemiconductor wafers 10 each with the coating film formed thereon isplaced on the lid 7 that has been moved down by the boat elevator 8.Then, the lid 7 is moved up by the boat elevator 8 to load thesemiconductor wafers 10 into the reaction tube 2. As a consequence, thesemiconductor wafers 10 are accommodated inside the inner tube 3 of thereaction tube 2, and the reaction tube 2 is airtightly closed.

After the reaction tube 2 is airtightly closed, the opening ratio of thevalve 18 is adjusted, and the vacuum pump 19 is driven to exhaust gasinside the reaction tube 2, thereby starting pressure reduction of thereaction tube 2. The interior of the reaction tube 2 is kept exhausteduntil the pressure inside the reaction tube 2 is reduced to apredetermined pressure.

After the interior of the reaction tube 2 is stabilized at thepredetermined pressure, a baking gas is supplied into the baking gasfeed line 13 at a predetermined flow rate from the baking gas supplysource of the gas supply section GS. The baking gas supplied into thebaking gas feed line 13 then flows through the heating device(activation section 14), where it is heated up to a temperature rangingfrom 700 to 1000° C., and thus activated. The activated baking gas iscontinuously supplied through the baking gas feed line 13 into thereaction tube 2 heated at the baking temperature. Under this state, thecoating film on the semiconductor wafers 10 is heated for apredetermined time, and thereby subjected to baking (heat process). As aconsequence, an inter-level insulating film (organosiloxane film) isformed on each semiconductor wafer 10.

The coating film on the semiconductor wafers 10 is subjected to baking(heat process) while the activated baking gas is supplied, so the bakingreaction of the coating film is promoted. In this case, even where theheat process temperature is set to be lower than a conventional valueranging from 400 to 450° C., the baking reaction sufficiently proceeds,whereby an inter-level insulating film with a low dielectric constant isformed. The baking temperature for the coating film is preferably set tobe not more than 400° C., such as a temperature ranging from 250 to 400°C., which is lower than the conventional heat process temperature. Ifthe heat process temperature is set to be lower than 250° C., the bakingreaction may insufficiently proceed, even where the activated baking gasis used.

Further, in this case, even where the heat process time is shortened,the baking reaction sufficiently proceeds, whereby an inter-levelinsulating film with a low dielectric constant is formed. It suffices ifthe heat process time is set at, e.g., 5 minutes or more. However, ifthe heat process time is too long, a film on the lower side may suffer aproblem related to a thermal history. For this reason, the heat processtime is preferably set at 60 minutes or less.

Returning to the explanation on steps of the heat-processing method,nitrogen is then supplied through the purge gas feed line 16 at apredetermined flow rate, while the opening ratio of the valve 18 isadjusted and the vacuum pump 19 is driven, to exhaust gas inside thereaction tube 2 through the exhaust line 17. It is preferable to performcyclic purge, in which the gas exhaust and nitrogen gas supply for theinterior of the process tube 2 are repeated a plurality of times, inorder to swiftly and reliably exhaust the gas inside the process tube 2.Subsequently, the pressure inside the process tube 2 is returned toatmospheric pressure, and the lid 7 is moved down by the boat elevator8, thus the semiconductor wafers 10 are unloaded.

In order to examine some of the effects of this embodiment, anexperiment was conducted to form an inter-level insulating film underdifferent conditions, and measure the specific dielectric constant ofthe film thus formed. More specifically, comparison was made between acase where a baking gas was activated immediately before being suppliedinto the reaction tube 2, and a case where the baking gas was notactivated, when semiconductor wafers 10 with a coating film formedthereon were subjected to a heat process (baking), using theheat-processing apparatus 1. In two present examples using an activatedbaking gas, ammonia gas and dinitrogen oxide gas were respectivelyemployed as the baking gas. In three comparative examples using anon-activated baking gas, nitrogen gas, ammonia gas, and dinitrogenoxide gas were respectively employed as the baking gas.

In each of the cases, the pressure inside the reaction tube 2 was set at13.3 kPa (100 Torr), the heat process temperature at 300° C., the heatprocess time at 30 minutes, and the flow rate of the baking gas at 0.5liters/minute. The coating film was formed by spin-coating a coatingsolution containing polysiloxane having an organic functional group ontoeach semiconductor wafer 10. After the heat process on the coating filmwas performed to form an inter-level insulating film, an electrodepattern consisting of aluminum or a mixture of aluminum and copper wasformed on the inter-level insulating film to form a sample. Then, thespecific dielectric constant of the inter-level insulating film of thissample was measured by a CV method, at a frequency of 100 kHz, using anLCR meter.

FIG. 2 is a graph showing the relationship between the bakingtemperature (heat process temperature) and the specific dielectricconstant of a film formed in a case where ammonia gas was employed asthe baking gas. FIG. 2 also shows data obtained in a case wherenon-activated nitrogen gas was employed (a gas conventionally employed).As show in FIG. 2, where activated ammonia gas was employed as thebaking gas, an inter-level insulating film with a low dielectricconstant was formed, although a lower baking temperature was used, ascompared with a case where non-activated nitrogen gas or non-activatedammonia gas was employed.

For example, the specific dielectric constant of an inter-levelinsulating film formed by baking with activated ammonia gas and a bakingtemperature of 300° C. was almost the same as the specific dielectricconstant of an inter-level insulating film formed by baking withnon-activated nitrogen gas and a baking temperature of 420° C. In otherwords, it was confirmed that, in spite of a lower baking temperature of300° C. being used for the coating film, ammonia gas used in accordancewith the heat process method according to this embodiment allowed aninter-level insulating film to be formed with a dielectric constant aslow as that obtained by the conventional technique. It is thought that alower baking temperature for the coating film enabled such aninter-level insulating film with a low dielectric constant to be formed,because the activated baking gas was supplied in baking the coating filmon the semiconductor wafers 10, thereby promoting the baking reaction ofthe coating film.

FIG. 3 is a graph showing the relationship between the bakingtemperature (heat process temperature) and the specific dielectricconstant of a film formed in a case where dinitrogen oxide gas wasemployed as the baking gas. FIG. 3 also shows data obtained in a casewhere non-activated nitrogen gas was employed (a gas conventionallyemployed). As show in FIG. 3, where activated dinitrogen oxide gas wasemployed as the baking gas, an inter-level insulating film with a lowdielectric constant was formed, although a lower baking temperature wasused, as compared with a case where non-activated nitrogen gas ornon-activated dinitrogen oxide gas was employed.

For example, the specific dielectric constant of an inter-levelinsulating film formed by baking with activated dinitrogen oxide gas anda baking temperature of 300° C. was almost the same as the specificdielectric constant of an inter-level insulating film formed by bakingwith non-activated nitrogen gas and a baking temperature of 420° C. Inother words, it was confirmed that, in spite of a lower bakingtemperature of 300° C. being used for the coating film, dinitrogen oxidegas used in accordance with the heat process method according to thisembodiment allowed an inter-level insulating film to be formed with adielectric constant as low as that obtained by the conventionaltechnique.

In order to study the influence of pressure on the specific dielectricconstant of an inter-level insulating film, an experiment was conducted.As a result, it was confirmed that the specific dielectric constant didnot substantially change with change in pressure.

The preferable supply rate of the baking gas differs, depending on thesize of the heat-processing apparatus 1 and the number of semiconductorwafers 10 to be loaded. For example, in the case of a heat-processingapparatus which employs a wafer boat 9 configured to load 170semiconductor wafers 10 of 8 inches at most, the supply rate of thebaking gas is preferably set to be within a range of from 0.01 to 10liters/minute, and more preferably within a range of from 0.1 to 2liters/minute.

As described above, according to this embodiment, the coating film onthe semiconductor wafers 10 is subjected to baking while the activatedbaking gas is supplied, so the baking reaction of the coating film ispromoted. As a consequence, even where the heat process temperature isset to be lower, an inter-level insulating film with a low dielectricconstant is formed.

The present invention is not limited to the embodiment described above,and it may be modified or applied in various manners. Next, anexplanation will be given of other possible embodiments of the presentinvention.

In the embodiment described above, a coating film is formed on asemiconductor wafer 10 by spin-coating a coating solution containingpolysiloxane having an organic functional group, and the coating filmthus formed is subjected to baking to form an inter-level insulatingfilm. For example, the coating solution containing polysiloxane havingan organic functional group is prepared by dissolving polysiloxanehaving an organic functional group into an organic solvent. Thissolution may contain an arbitrary component, such as a surfactant, addedthereto. An example of an inter-level insulating film thus formed is afilm of porous MSQ (methyl silsesquioxan) or MSQ. Where an inter-levelinsulating film consists of porous MSQ, the film includes pores with asize in molecular or atomic order, such as 20 nm or less, formedtherein.

In the embodiment described above, ammonia gas or dinitrogen oxide gasis used as a baking gas. However, another gas may be used as the bakinggas, as far as it can promote the baking reaction without affecting thebaking reaction. For example, the baking gas may consist of nitrogenoxide gas, hydrogen gas, argon gas, or nitrogen gas.

In the embodiment described above, the activation section 14 is formedof a heating device. However, the activation section 14 is merelyrequired to activate the baking gas. For example, the activation section14 may be formed of plasma generation means, photolyzation means,catalytic activation means, or a combination thereof.

In the embodiment described above, the processing apparatus isexemplified by a vertical heat-processing apparatus of the batch typewith the reaction tube 2 having a double-tube structure, which is formedof the inner tube 3 and outer tube 4. However, the present invention maybe applied to a heat-processing apparatus of the batch type with aprocess container having a single-tube structure, from which the innertube 3 is excluded. Alternatively, the present invention may be appliedto a heat-processing apparatus of the single-substrate type.

INDUSTRIAL APPLICABILITY

According to the present invention, where a polysiloxane based coatingfilm formed on a substrate is subjected to a heat process to form aninter-level insulating film, an inter-level insulating film with a lowdielectric constant can be formed even at a low heat processtemperature.

1. A method for processing an organosiloxane film, the methodcomprising: loading a target substrate with a coating film formedthereon into a reaction chamber, the coating film comprising apolysiloxane base solution having an organic functional group; andperforming a heat process on the target substrate within the reactionchamber to bake the coating film, wherein the heat process comprises atemperature setting step of setting an interior of the reaction chamberat a process temperature by heating, and a supplying step of supplying abaking gas into the reaction chamber set at the process temperature,while activating the baking gas by a gas activation section disposedoutside the reaction chamber.
 2. The method according to claim 1,wherein the process temperature ranges from 250 to 400° C.
 3. The methodaccording to claim 1, wherein the gas activation section is configuredto activate the baking gas by means of heat, light, plasma, or acatalyst.
 4. The method according to claim 1, wherein the baking gas isselected from the group consisting of ammonia gas, dinitrogen oxide gas,nitrogen oxide gas, hydrogen gas, argon gas, and nitrogen gas.
 5. Themethod according to claim 1, wherein the gas activation section isconfigured to activate the baking gas by bringing the baking gas intocontact with a catalyst, while supplying the baking gas with energy froma medium selected from the group consisting of heat, light, and plasma.6. The method according to claim 5, wherein the catalyst is selectedfrom the group consisting of tungsten, platinum, and titanium oxide. 7.An apparatus for processing an organosiloxane film, by performing a heatprocess on a target substrate with a coating film formed thereon to bakethe coating film, the coating film comprising a polysiloxane basesolution having an organic functional group, the apparatus comprising: areaction chamber configured to accommodate the target substrate; atemperature adjusting section configured to adjust temperature insidethe reaction chamber; a gas supply section configured to supply a bakinggas into the reaction chamber; a gas activation section disposed outsidethe reaction chamber and configured to activate the baking gas; anexhaust section configured to exhaust gas inside the reaction chamber;and a control section configured to control the temperature adjustingsection, the gas supply section, the gas activation section, and theexhaust section.
 8. The apparatus according to claim 7, wherein the gasactivation section is configured to activate the baking gas by means ofheat, light, plasma, or a catalyst.
 9. The apparatus according to claim7, wherein the baking gas is selected from the group consisting ofammonia gas, dinitrogen oxide gas, nitrogen oxide gas, hydrogen gas,argon gas, and nitrogen gas.
 10. The apparatus according to claim 7,wherein the gas activation section is configured to activate the bakinggas by bringing the baking gas into contact with a catalyst, whilesupplying the baking gas with energy from a medium selected from thegroup consisting of heat, light, and plasma.
 11. The apparatus accordingto claim 10, wherein the catalyst is selected from the group consistingof tungsten, platinum, and titanium oxide.
 12. The apparatus accordingto claim 7, wherein the control section is configure to execute the heatprocess to comprise a temperature setting step of setting an interior ofthe reaction chamber at a process temperature by heating, and asupplying step of supplying the baking gas into the reaction chamber setat the process temperature, while activating the baking gas by the gasactivation section disposed outside the reaction chamber.
 13. Theapparatus according to claim 7, wherein the process temperature rangesfrom 250 to 400° C.